CN106770199A - A kind of method that application ICP AES determine W content in molybdenum-iron - Google Patents
A kind of method that application ICP AES determine W content in molybdenum-iron Download PDFInfo
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Abstract
The invention discloses a kind of method that application ICP AES determine W content in molybdenum-iron, the method is：Step one, weigh molybdenum-iron sample；Step 2, prepare molybdenum-iron sample solution and molybdenum-iron sample blank solution；Step 3, preparation work curve solution；Step 4, using inductive coupling plasma emission spectrograph, the intensity of sequentially determining working curve solution, and with the concentration of working curve solution as abscissa, the intensity of working curve solution is ordinate, drawing curve；Step 5, drawing curve；Step 6, the W content determined in molybdenum-iron sample solution；W content in step 7, calculating molybdenum-iron sample.Measuring method of the invention has the advantages of consuming molybdenum-iron sample is few, and reliability is high, and precision is high, and finding speed is fast, easy to be accurate, sensitivity is high, while having good stability.
Description
Technical field
The invention belongs to analysis and testing technology field, and in particular to W content in a kind of application ICP-AES measure molybdenum-iron
Method.
Background technology
Molybdenum-iron is the alloy of molybdenum and iron, typically contains molybdenum 50~60%, the alloy addition as steel-making.Molybdenum-iron is to produce
Amorphous metal additive in journey, it has the several good characteristics for being delivered to new alloy.The key benefit of ferro-molybdenum it
One is its hardening capacity, makes the weldability of steel extremely strong, and molybdenum-iron is one of refractory metal.Additionally, increasing the alloy to molybdenum-iron
Corrosion resistance can be improved.The characteristic of the molybdenum-iron layer protecting film that caused it many on other metals, it is adaptable to various products.Molybdenum
Iron is also Legal Inspection commodity.
At present, although molybdenum-iron international standard (ISO5452-80) and domestic standard (ferroalloys of GB/T 3650 check and accept,
The general provision of packaging, accumulating, mark and quality certificate) in be not specified by the requirement of W content, standard GB/T/T
Also the method that W content is not determined in 5059 molybdenum-iron chemical analysis methods, but with expanding economy and the innovation of technology,
Quality requirement that can be progressively to molybdenum-iron product is improved, and may be related to the content requirement of wolfram element.At present, it is existing related public
Department is to the specific measurement data of W content requirement in molybdenum-iron, but the field also assay method without national standard.
Wolfram element can be incorporated into smelting iron and steel in molybdenum-iron, if energy quantitative analysis, the content of grasp tungsten, can improve molybdenum
The quality and range of application of iron, for this reason, it is necessary to the analysis to W content in molybdenum-iron is paid attention to and studied.Impurity unit in molybdenum-iron
Plain assay method is required for separating Mo substrate mostly, or using the means such as sheltering and eliminating the interference of molybdenum, more using drop
Determine traditional chemical analysis method such as method, volumetric method and AAS, the degree of accuracy of spectrophotometry and precision compared with
Low, measurement result is unstable, and measure detection limit is very high, while the cycle of measure is long, it is unfriendly to environment；And spectrographic determination process
Complexity, cost of determination is very high, and measurement range is narrow, and continuous mode is difficult to grasp and controls, and both approaches are all unsuitable for industry
Metaplasia quick requirement for determining in producing.Therefore, it is necessary to develop tungsten in a kind of suitable measure molybdenum-iron for producing inspection in enormous quantities contain
The method of amount.
The content of the invention
The technical problems to be solved by the invention are for above-mentioned the deficiencies in the prior art, there is provided one kind application ICP-
The method that AES determines W content in molybdenum-iron.The preparation method
In order to solve the above technical problems, the technical solution adopted by the present invention is：One kind application ICP-AES determines tungsten in molybdenum-iron
The method of content, it is characterised in that the method comprise the following steps for：
Step one, weigh molybdenum-iron sample：
0.2000~0.5000g molybdenum-iron samples are weighed, weighing is accurate to 0.0001g；
Step 2, prepare molybdenum-iron sample solution and molybdenum-iron sample blank solution：
Two identical beakers are taken, the molybdenum-iron sample weighed in step one, another beaker are put into one of beaker
In do not stride the molybdenum-iron sample weighed in rapid, then to the salpeter solution that same volume is separately added into two beakers, cover
The salpeter solution in two beakers is heated after surface plate until molybdenum-iron sample dissolves, then again to being separately added into phase in two beakers
The hydrochloric acid solution of same volume, removes the cooling of two beakers again after dissolving completely, when the solution in two beakers be cooled to room temperature it
Afterwards, beaker outer wall is rinsed with water, during the solution in two beakers then moved into two identical volumetric flasks respectively, finally uses water
Groove is diluted to, and is well mixed, molybdenum-iron sample solution and molybdenum-iron sample blank solution are obtained respectively；
Step 3, preparation work curve solution：
Weigh four parts of high-purity iron powders identical in quality to be respectively put into four identical beakers with high pure molybdenum powder, then at four
The salpeter solution of same volume is added in beaker, cap surface ware heats the salpeter solution in four beakers until high-purity iron powder and height
The dissolving of pure molybdenum powder, then to remove four beakers respectively to the hydrochloric acid solution that same volume is added in four beakers, after dissolving completely cold
But, after the solution in four beakers is cooled to room temperature, beaker outer wall is rinsed with water, then by the solution in four beakers point
0mL, 0.50mL, 1.00mL, 2.00mL tungsten standard liquid, dilute with water Yi Ru not be separately added into four identical volumetric flasks
To scale, it is well mixed, four parts of working curve solution is obtained；
Step 2 is identical with the addition volume of salpeter solution described in step 3 and hydrochloric acid solution；
Step 4, setting apparatus measures condition of work：
The measurement parameter of inductive coupling plasma emission spectrograph is set；
Step 5, drawing curve：
Distinguish determination step with the inductive coupling plasma emission spectrograph that measurement condition of work is set in step 4
The intensity of obtained four parts of working curve solution in three, measured intensity is made as ordinate with the concentration of tungsten standard liquid
It is abscissa, draws out working curve；
Step 6, the W content determined in molybdenum-iron sample solution：
Carrier gas is made with argon gas, with the inductive coupling plasma emission spectrograph that measurement condition of work is set in step 4
The intensity I of obtained molybdenum-iron sample solution in determination step two1, then obtained molybdenum-iron sample blank is molten in determination step two again
The intensity I of liquid2, then the working curve by being drawn from step 5 check in I1And I2The concentration ρ of tungsten is corresponded to respectively1And ρ2, ρ1With
ρ2Unit be mg/L；
Step 7, calculating：
W content in molybdenum-iron sample is with the mass fraction w of tungstenwRepresent, numerical value is represented with %, and according to equation below meter
Calculate：
Wherein V is the volume of molybdenum-iron sample solution, and unit is mL；M is to weigh the quality of molybdenum-iron sample, unit in step one
It is g.
The above-mentioned method for determining W content in molybdenum-iron, it is characterised in that salpeter solution described in step 2 and step 3
Addition volume be 10mL~20mL, the salpeter solution is by nitric acid and water according to (1~3):1 volume ratio is mixed；
The addition volume of hydrochloric acid solution described in step 2 and step 3 is 1mL~5mL, the hydrochloric acid solution by hydrochloric acid and water according to
(1~2):1 volume ratio is mixed, and the nitric acid and hydrochloric acid are guaranteed reagent.
The above-mentioned method for determining W content in molybdenum-iron, it is characterised in that heating for dissolving described in step 2 and step 3
Temperature be 150 DEG C~500 DEG C.
The above-mentioned method for determining W content in molybdenum-iron, it is characterised in that the body of beaker described in step 2 and step 3
Product is 100mL~200mL；The volume of the volumetric flask is 100mL.
The above-mentioned method for determining W content in molybdenum-iron, it is characterised in that the matter of the iron of high-purity iron powder described in step 3
Amount percentage composition is not less than 99.99%, and the weight/mass percentage composition of tungsten is less than 0.0001%；The quality hundred of molybdenum in the high pure molybdenum powder
Content is divided to be not less than 99.99%, the weight/mass percentage composition of tungsten is less than 0.0005%；The mass concentration of the tungsten standard liquid is
100mg/L；The volumetric flask volume is 100mL.
The above-mentioned method for determining W content in molybdenum-iron, it is characterised in that described in step 3 in high-purity iron powder iron matter
Amount with step one in weigh molybdenum-iron sample in iron it is identical in quality, in the molybdenum powder quality of molybdenum be step one in weighing molybdenum
Molybdenum in iron sample it is identical in quality.
The above-mentioned method for determining W content in molybdenum-iron, it is characterised in that inductively coupled plasma is set in step 4
The measurement parameter of emission spectrometer is specially：Radio-frequency power 1kW~1.5kW；20 μm of entrance slit；15 μm of exit slit；Cooling
Throughput 12L/min~15L/min；Sheath throughput 0.2L/min~0.3L/min；Time of integration 3s~10s；Selection
207.911nm spectral lines are used as measurement spectral line；Left and right background deduction value is zero.
The method of W content in above-mentioned molybdenum-iron, it is characterised in that the volumn concentration of argon gas described in step 6 is not
Less than 99.99%.
The present invention has advantages below compared with prior art：
1st, present invention application ICP-AES determines W content in molybdenum-iron, and the method sample pretreatment process need not be divided
From cumbersome operations such as, enrichments, the acid dissolving of simple two step is only needed in sample dissolving, separated without matrix, only need to be by molybdenum
Ferroelectric sample solution suction instrument is measured, and the content of tungsten in sample solution can be just shown after several tens of seconds.In this way
The content of tungsten in molybdenum-iron can directly be determined.The method minute is fast, and Determination Limit is low, determine precision it is high the characteristics of, fit
Quick detection and monitoring for product quality in production.
2nd, in the present invention measurement molybdenum-iron W content method is easy to operate, efficiency high, sensitivity are high, determine detection and be limited to
4.84mg/L, recovery of standard addition is 93.3%~103.7%, and measurement range is 0.0050%~0.1000%.The present invention is adapted to
Scientific research and industrial production, are especially more suitable for the quick industrialized production that determines.
Technical scheme is described in further detail below by embodiment.
Specific embodiment
Embodiment 1
The present embodiment application ICP-AES determine molybdenum-iron in W content method comprise the following steps for：
Step one, weigh molybdenum-iron sample：
Two, 0.2000g molybdenum-irons sample is weighed, weighing value is accurate to 0.0001g；
Step 2, prepare molybdenum-iron sample solution and molybdenum-iron sample blank solution：
Two beakers of 100mL are taken, the molybdenum-iron sample of the 0.2000g weighed in step one are put into one of beaker,
Do not striden in another beaker the molybdenum-iron sample weighed in rapid, it is then molten to the nitric acid that 10mL is separately added into two beakers
Liquid, is heated to 150 DEG C up to the dissolving of molybdenum-iron sample, then again to two after cap upper surface ware by the salpeter solution in two beakers
The hydrochloric acid solution of 1mL is separately added into beaker, two beaker coolings is removed after dissolving completely again, when the solution in two beakers is cold
But to after room temperature, beaker outer wall is rinsed with water, the solution in two beakers is then moved into two volumetric flasks of 100mL respectively
In, groove is finally diluted with water to, and be well mixed, molybdenum-iron sample solution and molybdenum-iron sample blank solution are obtained respectively；
Step 3, preparation work curve solution：
The high pure molybdenum powder of the high-purity iron powder and 0.1200g that weigh four parts of 0.0700g is respectively put into four beakers of 100mL
In, the salpeter solution of 10mL is then added in four beakers, the salpeter solution in two beakers is heated after cap upper surface ware
To 150 DEG C until high-purity iron powder and high pure molybdenum powder dissolve, then dissolved to the hydrochloric acid solution that 1mL is added in four beakers respectively
Four beaker coolings are removed after complete, after the solution in four beakers is cooled to room temperature, beaker outer wall is rinsed with water, then will
Solution in four beakers is moved into four volumetric flasks of 100mL respectively, is separately added into 0mL, 0.50mL, 1.00mL, 2.00mL
Tungsten standard liquid, is diluted with water to scale, is well mixed, and four parts of working curve solution are obtained；
Step 2 is with salpeter solution described in step 3 by nitric acid and water according to 1:1 volume ratio is mixed, described
Hydrochloric acid solution is by hydrochloric acid and water according to 1:1 volume ratio is mixed, and the nitric acid and hydrochloric acid are guaranteed reagent；
The weight/mass percentage composition of iron is not less than 99.99% in the high-purity iron powder, and the weight/mass percentage composition of tungsten is less than
0.0001%；The weight/mass percentage composition of molybdenum is not less than 99.99% in the high pure molybdenum powder, and the weight/mass percentage composition of tungsten is less than
0.0005%；The mass concentration of the tungsten standard liquid is 100mg/L；The volumetric flask volume is 100mL.
Step 4, setting apparatus measures condition of work：
The measurement parameter of inductive coupling plasma emission spectrograph is set；Inductively coupled plasma atomic emission is set
The measurement parameter of instrument is specially：Radio-frequency power 1kW；20 μm of entrance slit；15 μm of exit slit；Cooling gas flow 15L/min；Shield
Set throughput 0.2L/min；Time of integration 3s~10s；Selection 207.911nm spectral lines are used as measurement spectral line；Left and right background deduction value
It is zero.
Step 5, drawing curve：
Distinguish determination step with the inductive coupling plasma emission spectrograph that measurement condition of work is set in step 4
The intensity of obtained four parts of working curve solution in three, measured intensity is made as ordinate with the concentration of tungsten standard liquid
It is abscissa, draws out working curve；
Step 6, the W content determined in molybdenum-iron sample solution：
Carrier gas is made with argon gas, with the inductive coupling plasma emission spectrograph that measurement condition of work is set in step 4
The intensity I of obtained molybdenum-iron sample in determination step two1, then obtained molybdenum-iron sample blank solution in determination step two again
Intensity I2, then the working curve by being drawn from step 5 check in I1And I2The concentration ρ of tungsten is corresponded to respectively1And ρ2, unit is mg/
L；The volumn concentration of the argon gas is not less than 99.99%；
Step 7, the W content for calculating molybdenum-iron sample：
W content in molybdenum-iron sample is with the mass fraction w of tungstenwRepresent, numerical value is represented with %, and according to equation below meter
Calculate：
Wherein V is the volume of molybdenum-iron sample solution, and unit is mL；M is to weigh the quality of molybdenum-iron sample, unit in step one
It is g.Table 1 is the mass fraction W of tungsten in the molybdenum-iron for measuring above-mentioned measuring methodwResult.
Two molybdenum-iron samples are taken, 1 is respectively labeled as#Molybdenum-iron sample and 2#Molybdenum-iron sample, the step of according to embodiment 1 and side
Method is determined and calculated, 1 be calculated through the measuring method of embodiment 1 to repeating 7 times with portion molybdenum-iron sample respectively#Molybdenum
Iron sample and 2#The mass fraction of tungsten is w in molybdenum-iron samplew, the results are shown in Table 1.
Table 11#Molybdenum-iron sample and 2#The mass fraction w of tungsten in molybdenum-iron samplewMeasurement result
As it can be seen from table 1 the relative standard deviation (RSD) of measurement result calculated value is less than 1%, present invention measurement is illustrated
W content has good precision and stability in molybdenum-iron.
Measurement 1#Molybdenum-iron sample and 2#The recovery of standard addition of molybdenum-iron sample, two are moved into by the solution in two beakers respectively
After the volumetric flask of 100mL, a certain amount of tungsten standard substance is added, remaining presses the analytical procedure analysis of the present embodiment, adds tungsten mark
Result obtained by being determined after quasi- material subtracts sample original content, and its difference is sample with the ratio between theoretical value for adding standard substance
Recovery of standard addition, i.e.,：The recovery of standard addition of tungsten=(measuring original W content in total W content-sample in sample) ÷ adds
Enter amount × 100% of tungsten standard substance.Determine and result of calculation is shown in Table 2.As can be seen from Table 2, recovery of standard addition exists
More than 97%, illustrate that the present invention has the good degree of accuracy.
Table 21#Molybdenum-iron sample and 2#The mass fraction w of tungsten in molybdenum-iron samplewRecovery of standard addition
Embodiment 2
The present embodiment application ICP-AES determine molybdenum-iron in W content method comprise the following steps for：
Step one, weigh molybdenum-iron sample：
Two, 0.2500g molybdenum-irons sample is weighed, weighing value is accurate to 0.0001g；
Step 2, prepare molybdenum-iron sample solution and molybdenum-iron sample blank solution：
Two beakers of 150mL are taken, the molybdenum-iron sample of the 0.2500g weighed in step one are put into one of beaker,
Do not striden in another beaker the molybdenum-iron sample weighed in rapid, it is then molten to the nitric acid that 15mL is separately added into two beakers
Liquid, is heated to 150 DEG C up to the dissolving of molybdenum-iron sample, then again to two after cap upper surface ware by the salpeter solution in two beakers
The hydrochloric acid solution of 3mL is separately added into beaker, two beaker coolings is removed after dissolving completely again, when the solution in two beakers is cold
But to after room temperature, beaker outer wall is rinsed with water, the solution in two beakers is then moved into two volumetric flasks of 100mL respectively
In, groove is finally diluted with water to, and be well mixed, molybdenum-iron sample solution and molybdenum-iron sample blank solution are obtained respectively；
Step 3, preparation work curve solution：
The high pure molybdenum powder of the high-purity iron powder and 0.1500g that weigh four parts of 0.0900g is respectively put into four beakers of 100mL
In, the salpeter solution of 15mL is then added in four beakers, the salpeter solution in two beakers is heated after cap upper surface ware
To 150 DEG C until high-purity iron powder and high pure molybdenum powder dissolve, then dissolved to the hydrochloric acid solution that 3mL is added in four beakers respectively
Four beaker coolings are removed after complete, after the solution in four beakers is cooled to room temperature, beaker outer wall is rinsed with water, then will
Solution in four beakers is moved into four volumetric flasks of 100mL respectively, is separately added into 0mL, 0.50mL, 1.00mL, 2.00mL
Tungsten standard liquid, is diluted with water to scale, is well mixed, and four parts of working curve solution are obtained；
Salpeter solution described in step 2 and step 3 is by nitric acid and water according to 2:1 volume ratio is mixed, described
Hydrochloric acid solution is by hydrochloric acid and water according to 2:1 volume ratio is mixed, and the nitric acid and hydrochloric acid are guaranteed reagent；It is described
Nitric acid and hydrochloric acid are purchased in market, and the mass concentration of nitric acid is 65%~68%, and the mass concentration of hydrochloric acid is 36%~38%；
The weight/mass percentage composition of iron is not less than 99.99% in the high-purity iron powder, and the weight/mass percentage composition of tungsten is less than
0.0001%；The weight/mass percentage composition of molybdenum is not less than 99.99% in the high pure molybdenum powder, and the weight/mass percentage composition of tungsten is less than
0.0005%；The mass concentration of the tungsten standard liquid is 100mg/L；The volumetric flask volume is 100mL；
Step 4, setting apparatus measures condition of work：
The measurement parameter of inductive coupling plasma emission spectrograph is set；Inductively coupled plasma atomic emission is set
The measurement parameter of instrument is specially：Radio-frequency power 1.2kW；20 μm of entrance slit；15 μm of exit slit；Cooling gas flow 13L/min；
Sheath throughput 0.25L/min；Time of integration 3s~8s；Selection 207.911nm spectral lines are used as measurement spectral line；Left and right background deduction
Value is zero.
Step 5, drawing curve：
Distinguish determination step with the inductive coupling plasma emission spectrograph that measurement condition of work is set in step 4
The intensity of obtained four parts of working curve solution in three, measured intensity is made as ordinate with the concentration of tungsten standard liquid
It is abscissa, draws out working curve；
Step 6, the W content determined in molybdenum-iron sample solution：
Carrier gas is made with argon gas, with the inductive coupling plasma emission spectrograph that measurement condition of work is set in step 4
The intensity I of obtained molybdenum-iron sample in determination step two1, then obtained molybdenum-iron sample blank solution in determination step two again
Intensity I2, then the working curve by being drawn from step 5 check in I1And I2The concentration ρ of tungsten is corresponded to respectively1And ρ2, unit is mg/
L；The volumn concentration of the argon gas is not less than 99.99%；
Step 7, calculating：
W content in molybdenum-iron sample is with the mass fraction w of tungstenwRepresent, numerical value is represented with %, and according to equation below meter
Calculate：
Wherein V is the volume of molybdenum-iron sample solution, and unit is mL；M is to weigh the quality of molybdenum-iron sample, unit in step one
It is g.Table 1 is the mass fraction W of tungsten in the molybdenum-iron for measuring above-mentioned measuring methodwResult.
Two molybdenum-iron samples are taken, 3 are respectively labeled as#Molybdenum-iron sample and 4#Molybdenum-iron sample, the step of according to embodiment 1 and side
Method is determined and calculated, 3 be calculated through the measuring method of the present embodiment to repeating 7 times with portion molybdenum-iron sample respectively#
Molybdenum-iron sample and 4#The mass fraction of tungsten is w in molybdenum-iron samplew, the results are shown in Table 3.
Table 33#Molybdenum-iron sample and 4#The mass fraction w of tungsten in molybdenum-iron samplewMeasurement result
From table 3 it can be seen that the relative standard deviation (RSD) of measurement result calculated value is less than 1%, present invention measurement is illustrated
W content has good precision and stability in molybdenum-iron.
Measurement 3#Molybdenum-iron sample and 4#The recovery of standard addition of molybdenum-iron sample, by the solution difference in two beakers in step 2
After moving into two volumetric flasks of 100mL, a certain amount of tungsten standard substance is added, remaining presses the analytical procedure analysis of the present embodiment,
Result obtained by being determined after addition tungsten standard substance subtracts sample original content, and its difference is with the ratio between theoretical value for adding standard substance
As sample recovery of standard addition, i.e.,：The recovery of standard addition of tungsten=(original tungsten contains in measuring total W content-sample in sample
Amount) ÷ add tungsten standard substance amount × 100%.Determine and result of calculation is shown in Table 4.As can be seen from Table 4, mark-on reclaims
Rate illustrates that the present invention has the good degree of accuracy more than 97%.
Table 43#Molybdenum-iron sample and 4#The mass fraction w of tungsten in molybdenum-iron samplewRecovery of standard addition
Embodiment 3
The present embodiment application ICP-AES determine molybdenum-iron in W content method comprise the following steps for：
Step one, weigh molybdenum-iron sample：
Two, 0.5000g molybdenum-irons sample is weighed, weighing value is accurate to 0.0001g；
Step 2, prepare molybdenum-iron sample solution and molybdenum-iron sample blank solution：
Two beakers of 200mL are taken, the molybdenum-iron sample of the 0.5000g weighed in step one are put into one of beaker,
Do not striden in another beaker the molybdenum-iron sample weighed in rapid, it is then molten to the nitric acid that 20mL is separately added into two beakers
Liquid, is heated to 150 DEG C up to the dissolving of molybdenum-iron sample, then again to two after cap upper surface ware by the salpeter solution in two beakers
The hydrochloric acid solution of 5mL is separately added into beaker, two beaker coolings is removed after dissolving completely again, when the solution in two beakers is cold
But to after room temperature, beaker outer wall is rinsed with water, the solution in two beakers is then moved into two volumetric flasks of 100mL respectively
In, groove is finally diluted with water to, and be well mixed, molybdenum-iron sample solution and molybdenum-iron sample blank solution are obtained respectively；
Step 3, preparation work curve solution：
The high pure molybdenum powder of the high-purity iron powder and 0.1500g that weigh four parts of 0.0900g is respectively put into four beakers of 100mL
In, the salpeter solution of 20mL is then added in four beakers, the salpeter solution in two beakers is heated after cap upper surface ware
To 150 DEG C until high-purity iron powder and high pure molybdenum powder dissolve, then dissolved to the hydrochloric acid solution that 5mL is added in four beakers respectively
Four beaker coolings are removed after complete, after the solution in four beakers is cooled to room temperature, beaker outer wall is rinsed with water, then will
Solution in four beakers is moved into four volumetric flasks of 100mL respectively, is separately added into 0mL, 0.50mL, 1.00mL, 2.00mL
Tungsten standard liquid, is diluted with water to scale, is well mixed, and four parts of working curve solution are obtained；
Salpeter solution described in step 2 and step 3 is by nitric acid and water according to 3:1 volume ratio is mixed, described
Hydrochloric acid solution is by hydrochloric acid and water according to 3:1 volume ratio is mixed, and the nitric acid and hydrochloric acid are guaranteed reagent；
The weight/mass percentage composition of the iron of the high-purity iron powder is not less than 99.99%, and the weight/mass percentage composition of tungsten is less than
0.0001%；The weight/mass percentage composition of molybdenum is not less than 99.99% in the high pure molybdenum powder, and the weight/mass percentage composition of tungsten is less than
0.0005%；The mass concentration of the tungsten standard liquid is 100mg/L；The volumetric flask volume is 100mL；
Step 4, setting apparatus measures condition of work：
The measurement parameter of inductive coupling plasma emission spectrograph is set；Inductively coupled plasma atomic emission is set
The measurement parameter of instrument is specially：Radio-frequency power 1.5kW；20 μm of entrance slit；15 μm of exit slit；Cooling gas flow 12L/min；
Sheath throughput 0.2L/min；Time of integration 5s；Selection 207.911nm spectral lines are used as measurement spectral line；Left and right background deduction value is
Zero.
Step 5, drawing curve：
Distinguish determination step with the inductive coupling plasma emission spectrograph that measurement condition of work is set in step 4
The intensity of obtained four parts of working curve solution in three, measured intensity is made as ordinate with the concentration of tungsten standard liquid
It is abscissa, draws out working curve；
Step 6, the W content determined in molybdenum-iron sample solution：
Carrier gas is made with argon gas, with the inductive coupling plasma emission spectrograph that measurement condition of work is set in step 4
The intensity I of obtained molybdenum-iron sample solution in determination step two1, then obtained molybdenum-iron sample blank is molten in determination step two again
The intensity I of liquid2, then the working curve by being drawn from step 5 check in I1And I2The concentration ρ of tungsten is corresponded to respectively1And ρ2, unit
It is mg/L；The volumn concentration of the argon gas is not less than 99.99%；
Step 7, calculating：
W content in molybdenum-iron sample is with the mass fraction w of tungstenwRepresent, numerical value is represented with %, and according to equation below meter
Calculate：
Wherein V is the volume of molybdenum-iron sample solution, and unit is mL；M is to weigh the quality of molybdenum-iron sample, unit in step one
It is g.Table 1 is the mass fraction W of tungsten in the molybdenum-iron for measuring above-mentioned measuring methodwResult.
Two molybdenum-iron samples are taken, 5 are respectively labeled as#Molybdenum-iron sample and 6#Molybdenum-iron sample, the step of according to embodiment 1 and side
Method is determined and calculated, 5 be calculated through the measuring method of the present embodiment to repeating 7 times with portion molybdenum-iron sample respectively#
Molybdenum-iron sample and 6#The mass fraction of tungsten is w in molybdenum-iron samplew, the results are shown in Table 5.
Table 55#Molybdenum-iron sample and 6#The mass fraction w of tungsten in molybdenum-iron samplewMeasurement result
As can be seen from Table 5, the relative standard deviation (RSD) of measurement result calculated value is less than 1%, illustrates present invention measurement
W content has good precision and stability in molybdenum-iron.
Measurement 5#Molybdenum-iron sample and 6#The recovery of standard addition of molybdenum-iron sample, by the solution difference in two beakers in step 2
After moving into two volumetric flasks of 100mL, a certain amount of tungsten standard substance is added, remaining presses the analytical procedure analysis of the present embodiment,
Result obtained by being determined after addition tungsten standard substance subtracts sample original content, and its difference is with the ratio between theoretical value for adding standard substance
As sample recovery of standard addition, i.e.,：The recovery of standard addition of tungsten=(original tungsten contains in measuring total W content-sample in sample
Amount) ÷ add tungsten standard substance amount × 100%.Determine and result of calculation is shown in Table 6.As can be seen from Table 6, mark-on reclaims
Rate illustrates that the present invention has the good degree of accuracy more than 90%.
Table 65#Molybdenum-iron sample and 6#The mass fraction w of tungsten in molybdenum-iron samplewRecovery of standard addition
The above, is only presently preferred embodiments of the present invention, and not the present invention is imposed any restrictions.It is every according to invention skill
Any simple modification, change and equivalence change that art is substantially made to above example, still fall within technical solution of the present invention
Protection domain in.
Claims (8)
1. a kind of method that application ICP-AES determines W content in molybdenum-iron, it is characterised in that the method comprise the following steps for：
Step one, weigh molybdenum-iron sample：
0.2000~0.5000g molybdenum-iron samples are weighed, weighing is accurate to 0.0001g；
Step 2, prepare molybdenum-iron sample solution and molybdenum-iron sample blank solution：
Two identical beakers are taken, the molybdenum-iron sample weighed in step one is put into one of beaker, in another beaker not
Stride the molybdenum-iron sample weighed in rapid, then to the salpeter solution that same volume is separately added into two beakers, cap upper surface
The salpeter solution in two beakers is heated after ware until molybdenum-iron sample dissolves, then again to being separately added into same volume in two beakers
Long-pending hydrochloric acid solution, removes two beaker coolings again after dissolving completely, after the solution in two beakers is cooled to room temperature, use
Water rinses beaker outer wall, during the solution in two beakers then moved into two identical volumetric flasks respectively, last dilute with water
To groove, and it is well mixed, molybdenum-iron sample solution and molybdenum-iron sample blank solution is obtained respectively；
Step 3, preparation work curve solution：
Weigh four parts of high-purity iron powders identical in quality to be respectively put into four identical beakers with high pure molybdenum powder, then in four beakers
The salpeter solution of middle addition same volume, cap surface ware heats the salpeter solution in four beakers until high-purity iron powder and High-Purity Molybdenum
Powder dissolves, then respectively to the hydrochloric acid solution that same volume is added in four beakers, four beaker coolings is removed after dissolving completely, when
Solution in four beakers is cooled to after room temperature, and beaker outer wall is rinsed with water, then moves the solution in four beakers respectively
Enter in four identical volumetric flasks, be separately added into 0mL, 0.50mL, 1.00mL, 2.00mL tungsten standard liquid, be diluted with water to quarter
Degree, is well mixed, and four parts of working curve solution are obtained；
Step 2 is identical with the addition volume of salpeter solution described in step 3 and hydrochloric acid solution；
Step 4, setting apparatus measures condition of work：
The measurement parameter of inductive coupling plasma emission spectrograph is set；
Step 5, drawing curve：
With set in step 4 measurement condition of work inductive coupling plasma emission spectrograph distinguish determination step three in
The intensity of obtained four parts of working curve solution, measured intensity as ordinate, using the concentration of tungsten standard liquid as horizontal stroke
Coordinate, draws out working curve；
Step 6, the W content determined in molybdenum-iron sample solution：
Carrier gas is made with argon gas, is determined with the inductive coupling plasma emission spectrograph that measurement condition of work is set in step 4
The intensity I of obtained molybdenum-iron sample solution in step 21, then obtained molybdenum-iron sample blank solution in determination step two again
Intensity I2, then the working curve by being drawn from step 5 check in I1And I2The concentration ρ of tungsten is corresponded to respectively1And ρ2, ρ1And ρ2's
Unit is mg/L；
Step 7, the W content calculated in molybdenum-iron sample：
W content in molybdenum-iron sample is with the mass fraction w of tungstenwRepresent, numerical value is represented with %, and calculated according to equation below：
Wherein V is the volume of molybdenum-iron sample solution, and unit is mL；M is to weigh the quality of molybdenum-iron sample in step one, and unit is g.
2. it is according to claim 1 determine molybdenum-iron in W content method, it is characterised in that institute in step 2 and step 3
The addition volume for stating salpeter solution is 10mL~20mL, and the salpeter solution is by nitric acid and water according to (1~3):1 volume ratio
Mix；The addition volume of hydrochloric acid solution described in step 2 and step 3 is 1mL~5mL, and the hydrochloric acid solution is by salt
Acid is with water according to (1~2):1 volume ratio is mixed, and the nitric acid and hydrochloric acid are guaranteed reagent.
3. it is according to claim 1 determine molybdenum-iron in W content method, it is characterised in that institute in step 2 and step 3
The temperature for stating heating for dissolving is 150 DEG C~500 DEG C.
4. it is according to claim 1 determine molybdenum-iron in W content method, it is characterised in that institute in step 2 and step 3
The volume for stating beaker is 100mL~200mL；The volume of the volumetric flask is 100mL.
5. it is according to claim 1 determine molybdenum-iron in W content method, it is characterised in that high purity iron described in step 3
The weight/mass percentage composition of the iron of powder is not less than 99.99%, and the weight/mass percentage composition of tungsten is less than 0.0001%；In the high pure molybdenum powder
The weight/mass percentage composition of molybdenum is not less than 99.99%, and the weight/mass percentage composition of tungsten is less than 0.0005%；The matter of the tungsten standard liquid
Amount concentration is 100mg/L；The volumetric flask volume is 100mL.
6. it is according to claim 1 determine molybdenum-iron in W content method, it is characterised in that high purity iron described in step 3
Iron is identical in quality in the molybdenum-iron sample weighed in the quality of iron and step one in powder, and the quality of molybdenum is step one in the molybdenum powder
Molybdenum in the molybdenum-iron sample of middle weighing it is identical in quality.
7. it is according to claim 1 determine molybdenum-iron in W content method, it is characterised in that in step 4 set inductance coupling
The measurement parameter for closing plasma emission spectrometer is specially：Radio-frequency power 1kW~1.5kW；20 μm of entrance slit；Exit slit
15μm；Cooling gas flow 12L/min~15L/min；Sheath throughput 0.2L/min~0.3L/min；Time of integration 3s~10s；
Selection 207.911nm spectral lines are used as measurement spectral line；Left and right background deduction value is zero.
8. in molybdenum-iron according to claim 1 W content method, it is characterised in that the volume of argon gas described in step 6
Percentage composition is not less than 99.99%.
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| CN111272738A (en) * | 2020-03-04 | 2020-06-12 | 首钢京唐钢铁联合有限责任公司 | Method for detecting content of trace elements in zinc-aluminum-magnesium alloy |
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